CN115219604B - Method for detecting fat-soluble vitamins in infant milk powder - Google Patents
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Abstract
The invention provides a method for detecting fat-soluble vitamins in infant milk powder, which adopts liquid chromatography-mass spectrometry to simultaneously detect the content of the vitamins in infant milk powder, and comprises the following steps: (1) pre-treating a milk powder sample to be tested; (2) preparing a standard working solution for establishing a standard curve; (3) Detecting a milk powder sample to be detected by adopting a liquid chromatograph-tandem mass spectrometer; wherein the fat-soluble vitamins include vitamin A and vitamin D 3 Vitamin E and vitamin K 1 The method comprises the steps of carrying out a first treatment on the surface of the Conditions of the liquid chromatography: adopting a gradient elution mode, and a mobile phase A: 0.1.+ -. 0.05% formic acid solution, mobile phase B: 1.+ -. 0.1% methylene chloride in methanol. The method can rapidly and simultaneously detect the contents of various fat-soluble vitamins in the milk powder, has higher accuracy and precision, can simplify the sample processing steps, and improves the detection efficiency.
Description
Technical Field
The invention relates to the technical field of food detection, in particular to a method for detecting fat-soluble vitamins in infant milk powder.
Background
Infant formula as a main food source for non-breast-fed infants must contain all the nutrients it grows and develops, and fat-soluble vitamins as the main nutrients in it are essential for infants to perform normal metabolism. Vitamin a deficiency, for example, can lead to blindness in children and affect the prevalence and mortality of childhood infectious diseases; vitamin D deficiency can cause disturbance of calcium and phosphorus metabolism, affect bones, and cause systemic chronic nutritional diseases of infants closely related to life style and characterized by skeletal lesions; vitamin E deficiency can lead to abnormalities in the human reproductive system, the muscular system, the cardiovascular system and the hematopoietic system. Therefore, strict product standards are formulated for the products in China, such as GB 10765-2010 food safety national standard infant formula and GB10767-2010 food safety national standard older infant and infant formula.
Instrument prescription for measuring fat-soluble vitaminsThe method comprises normal phase chromatography, reversed phase chromatography, liquid chromatography-tandem mass spectrometry and the like, wherein vitamin A and vitamin D have ultraviolet absorption groups, and vitamin E has both ultraviolet absorption groups and fluorescence response, so that the detection can be carried out simultaneously under the liquid phase condition. But vitamin K 1 Because of no ultraviolet absorbing group, the detection is carried out after reduction by using a zinc powder reduction column, so that the 4 lipid-soluble vitamins cannot be analyzed by liquid chromatography at the same time. For determining fat-soluble vitamins including vitamin A, vitamin E, vitamin D and vitamin K 1 2 national method standards of (a) are GB 5009.82-2016 and GB5009.158-2016 respectively; there are also 3 AOAC methods for the determination of these 4 fat-soluble vitamins, AOAC 2012.10 for the detection of vitamin A and vitamin E, AOAC 2016.05 for the detection of vitamin D, and AOAC 2015.09 for the detection of vitamin K, respectively 1 . When the method is used for detection, the samples are subjected to differentiation treatment according to different detection items, the treatment process is complex, the enzymolysis, saponification, liquid-liquid extraction, water washing, desolventizing, re-dissolving and other processes are often needed, and meanwhile, a plurality of sets of equipment are needed for qualitative and quantitative analysis, so that time and labor are wasted, and resources are occupied. Therefore, there is a need for a better detection method to simplify the sample pretreatment steps and improve the sample processing capacity.
Disclosure of Invention
In order to improve the processing capacity of milk powder samples and improve the detection efficiency, the invention provides a method for simultaneously detecting 4 lipid-soluble vitamins in infant milk powder by using liquid chromatography-tandem mass spectrometry. The method has high detection efficiency, and can detect 4 lipid-soluble vitamins simultaneously.
The technical scheme of the invention is as follows: a method for detecting fat-soluble vitamins in infant milk powder adopts liquid chromatography-mass spectrometry to simultaneously detect the content of the vitamins in infant milk powder, and comprises the following steps:
(1) Pre-treating a milk powder sample to be tested;
(2) Preparing standard working solution for establishing a standard curve;
(3) Detecting a milk powder sample to be detected by adopting a liquid chromatograph-tandem mass spectrometer;
wherein the fat-soluble vitamins include vitamin A and vitamin D 3 Vitamin E and vitamin K 1 ；
Conditions of the liquid chromatography: adopting a gradient elution mode, and a mobile phase A: 0.1.+ -. 0.05% formic acid solution, mobile phase B: 1.+ -. 0.1% methylene chloride in methanol.
Further, the vitamin A also comprises the existence form of vitamin A palmitate and vitamin A acetate, and the vitamin E also comprises the existence form of vitamin E acetate.
Further, the gradient elution mode specifically includes: 0 to 0.5 minutes, 20 percent of A is kept unchanged; 0.5-4 minutes, 20% A is linearly changed to 0% A; 4-8.5 minutes, 0% A remains unchanged; 8.51 min change to 20% A, hold for 2min.
Further, the mass spectrometry conditions were: an atmospheric pressure chemical ionization ion source (APCI), positive ionization mode, ion pairs and collision energy parameters of the mass spectrum are specifically shown in the following table;
further, the milk powder to be tested is subjected to pretreatment, and the pretreatment step comprises the following steps: accurately weighing a milk powder sample to be measured, adding a proper amount of antioxidant, dissolving with water, adding methanol to precipitate protein, and extracting fat-soluble vitamins from the milk powder sample by using an organic extraction solvent; centrifuging, taking upper layer solution, blowing nitrogen to dry, performing solvent conversion by using a double-dissolving solvent, and filtering to obtain the liquid to be detected.
Further, the extraction solvent is isooctane.
Further, the redissolution solvent is acetone.
Further, after conversion with a redissolved solvent, filtration was performed with an organic filter membrane having a thickness of 0.22 μm.
According to the method for detecting the fat-soluble vitamins in the infant milk powder, a standard curve is established by adopting an external standard method, and the method specifically comprises the following steps: preparing vitamin A, vitamin A palmitate, vitamin A acetate and vitamin D 3 Vitamin E, vitamin E acetate and vitamin K 1 The standard working solution of (2) is detected by a liquid chromatograph-tandem mass spectrometer, the chromatographic peak area of each fat-soluble vitamin is taken as the ordinate, the concentration is taken as the abscissa, and the standard curve of each vitamin is drawn.
The invention has the beneficial effects that: (1) According to the invention, the liquid chromatography-tandem mass spectrometry is used for simultaneously detecting the 4 lipoid soluble vitamins in the infant milk powder, so that the sample pretreatment steps are simplified, and the sample treatment capacity is improved; (2) Through optimizing and improving the detection conditions, the peak time of each vitamin is shortened, the detection efficiency of the sample is greatly improved, and the accuracy is higher.
Drawings
FIG. 1 is a liquid chromatography-tandem mass spectrometry chromatogram of each lipid-soluble vitamin standard;
fig. 2 is a liquid chromatography-tandem mass spectrometry chromatogram of each fat-soluble vitamin of the milk powder sample to be tested.
Detailed Description
The technical means adopted by the invention and the effects thereof are further described below with reference to the examples and the attached drawings. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting thereof.
Reagents, materials and instrumentation used in the following examples are described below.
Reagents and materials: standard vitamin A, vitamin A palmitate, vitamin acetate, vitamin E acetate, vitamin D 3 Vitamin K 1 And dibutylhydroxytoluene (BHT) from Sigma; dichloromethane, methanol, acetonitrile, isopropanol, formic acid were chromatographically pure, purchased from Fisher Scientific; n-hexane, cyclohexane, diethyl ether, petroleum ether, methyl tert-butyl ether, isooctane and acetoneChemical purity, purchased from national pharmaceutical and chemical reagents, inc; ultrapure water is produced by a Millipore Milli-Q ultrapure water meter.
Instrument and apparatus: a Waters XEVO TQXS liquid chromatograph-tandem mass spectrometer equipped with an atmospheric pressure chemical ionization ion source (APCI); eppendorf 5804 centrifuge; WIGGENS Vortex 3000 Vortex oscillator.
In the following examples, the standard solution is a mother solution prepared from each of the fat-soluble vitamin standards; the blank matrix solution is a milk powder sample solution without an object to be detected; the standard working solution with a certain concentration can be obtained by diluting the standard solution with the blank matrix solution.
The invention provides a method for detecting fat-soluble vitamins in infant milk powder, which adopts a liquid chromatography-mass spectrometry method to detect the content of the vitamins in the infant milk powder and comprises the following steps: (1) pre-treating a milk powder sample to be tested; (2) preparing a standard working solution for establishing a standard curve; (3) Detecting a milk powder sample to be detected by adopting a liquid chromatograph-tandem mass spectrometer;
wherein, the liquid chromatography adopts a gradient elution mode;
the specific steps of pre-treating the milk powder sample to be tested are as follows: accurately weighing a milk powder sample to be measured, adding a proper amount of antioxidant, dissolving with water, adding methanol to precipitate protein, and extracting fat-soluble vitamins from the milk powder sample by using an organic extraction solvent; centrifuging, taking upper layer solution, blowing nitrogen to dry, performing solvent conversion by using a double-dissolving solvent, and filtering to obtain the liquid to be detected.
In order to obtain a method for simultaneously detecting 4 lipoid-soluble vitamins in infant milk powder by using liquid chromatography-tandem mass spectrometry, the inventor firstly screens and optimizes detection conditions, and specifically comprises the following steps.
Example 1 influence of different flows on detection results in liquid chromatography
Experiments show that the solvents such as methanol, acetonitrile and the like are used as flowing relative vitamins A, vitamin A palmitate, vitamin A acetate, vitamin E acetate and vitamin D 3 And vitamin K 1 At C 18 The elution capacity on the chromatographic column, the liquid to be measured is the standard working liquid of each fat-soluble vitamin.Experiments show that when acetonitrile is used as a mobile phase, the eluting capability of the vitamin A palmitate is weak, so that the peak-off time is overlong; when methanol is used as the mobile phase, the eluting power of methanol is higher than that of acetonitrile, but the peak time is still longer than 10 minutes, and the detection efficiency is still lower.
In order to strengthen the eluting capability of the mobile phase, a small amount of methylene dichloride is added into methanol of the mobile phase, and when the methylene dichloride content is increased to about 1%, the peak time of the vitamin A palmitate can be obviously improved, the detected peak time of each vitamin is reduced to be within 10 minutes, and the peak of each vitamin is sharpened; considering the influence of dichloromethane on the body of staff, the dichloromethane needs to be as little as possible, so that the addition amount of the dichloromethane needs to be preferentially selected; meanwhile, in order to ensure that the vitamin A and the vitamin A acetate do not peak too early, proper water is added in the initial stage to increase the polarity of the mobile phase, so that the optimized preferred chromatographic condition mobile phase combination is as follows: 0.1.+ -. 0.05% formic acid in water and 1.+ -. 0.1% methylene chloride-methanol.
Under the preferable liquid chromatography condition, the chromatogram of each standard working solution of the fat-soluble vitamins is shown in figure 1, each detected fat-soluble vitamin can show a peak within 10 minutes, and the specific peak position of each fat-soluble vitamin can be determined according to figure 1, wherein three peaks in the chromatogram of vitamin A are vitamin A, vitamin A acetate and vitamin A palmitate in sequence.
Example 2 Effect of different extraction solvents on extraction Effect
In the pretreatment step of the milk powder sample to be tested, different extraction solvents are adopted, and diethyl ether is examined: petroleum ether (1:1, v:v), n-hexane: cyclohexane: diethyl ether (4:4:2, v:v:v) n-hexane isooctane, etc. as extraction solvent, the liquid to be measured obtained by using different extraction solvents was detected by a liquid chromatograph tandem mass spectrometer, and the results are shown in table 1.
TABLE 1 extraction Effect of extraction solvent
The detection results showed that when diethyl ether was used: petroleum ether (1:1, v:v) and n-hexane: cyclohexane: diethyl ether' 4:4:2, v:v:v a) in the case of a system, after centrifugation, a thicker emulsifying layer exists between the water phase and the organic phase, so that the test result is lower; when n-hexane or isooctane is used, the aqueous phase and the organic phase can be separated well after centrifugation, but the extraction efficiency of n-hexane is lower than that of isooctane, so that isooctane is preferable as the extraction solvent in the end.
EXAMPLE 3 Effect of different reconstitution solvents on extraction Effect
In the pretreatment step of the sample to be tested, the extraction solvent isooctane solution cannot directly enter the reversed phase chromatographic system, so that the solvent conversion is required before the sample injection test. Experiments have compared the re-dissolution effects of different re-dissolution solvents such as isopropanol, methanol, acetonitrile and acetone, and the experiments show that when the isopropanol, the methanol and the acetonitrile are used for re-dissolution, the residue after nitrogen blowing cannot be completely dissolved, the solution is turbid, and when the acetone is used as the re-dissolution solvent, the residue can be completely dissolved, so that the acetone is preferably used as the re-dissolution solvent.
According to the screening and optimization of the detection conditions in the above embodiments, the preferred conditions for detecting the fat-soluble vitamins in infant milk powder by using liquid chromatography tandem mass spectrometry are determined. In mobile phase selection for liquid chromatography, mobile phase a: 0.1.+ -. 0.05% formic acid solution, mobile phase B: 1+/-0.1% methylene dichloride methanol solution; in the pretreatment of the milk powder sample to be tested, preferably, isooctane is used as an extraction solvent to extract vitamins, and acetone is used as a redissolution solvent to perform solvent conversion.
The detection method of the present invention is further verified by the following specific examples.
Example 4 milk powder sample detection method
1. Liquid chromatography conditions:
chromatographic column model: waters BEH C 18 2.1×50mm，1.7μm；
Mobile phase a:0.1% formic acid solution;
mobile phase B:1% methylene chloride in methanol;
column temperature: 40 ℃, flow rate: sample injection amount of 0.5 mL/min: 2. Mu.L;
adopts a gradient elution mode: 0 to 0.5 minutes, 20 percent of A is kept unchanged; 0.5-4 minutes, 20% A is linearly changed to 0% A; 4-8.5 minutes, 0% A remains unchanged; 8.51 min change to 20% A, hold for 2min.
2. Mass spectrometry conditions:
atmospheric pressure chemical ionization ion source (APCI), positive ionization mode; corona current: 15.0 μA; taper hole voltage: 30V; ion source temperature: 400 ℃; drying gas flow rate: 800L/hr; taper hole reverse blowing flow rate: 150L/hr. The mass spectrum parameter ion pairs and collision energy of each substance to be tested are shown in table 2.
Table 2 mass spectral parameters
3. Preparation of standard working solution
Vitamin A, vitamin A palmitate, vitamin A acetate, vitamin E acetate, vitamin D were formulated at the same concentrations using standard samples 3 Vitamin K 1 And diluting each standard solution into standard working solutions with different concentrations by using a blank matrix solution, wherein the prepared standard working solution can be used for establishing a standard curve. In this example, the standard solutions of each vitamin were diluted into 6 groups of standard working solutions having different concentrations, and the concentrations of the standard working solutions of each fat-soluble vitamin are shown in table 3.
TABLE 3 Standard working solution concentrations of fat-soluble vitamins
4. Pretreatment of milk powder sample to be tested
Accurately weighing 0.500g of sample milk powder, adding 0.1g of antioxidant BHT, adding 10mL of water, mixing by vortex, adding 20mL of methanol, standing for 10min after vortex for 20 seconds, adding 10mL of isooctane, vortex for 20 seconds, and centrifuging at 9000rpm for 2min. Taking 1mL of supernatant, blowing nitrogen in a water bath at 40 ℃ to dry, re-dissolving the supernatant by using acetone, filtering the supernatant by using an organic filter membrane with the thickness of 0.22 mu m to obtain a liquid to be detected, and carrying out sample analysis.
The liquid chromatograph-tandem mass spectrometer is used for detecting the treated liquid to be detected, the detection result is shown in figure 2, each fat-soluble vitamin in the milk powder can show a peak within 10 minutes, and 4 fat-soluble vitamins can be rapidly detected, and the vitamin D in the sample can be detected 3 In the chromatogram of (2), the arrow in the figure indicates vitamin D 3 Is the peak position of the (c).
Example 5 verification of the detection method
1. Linear relationship and quantitative limit
The standard curve is established by an external standard method, specifically, liquid chromatography-tandem mass spectrometry detection analysis is carried out on standard working solutions with different concentrations of each fat-soluble vitamin in table 3, the standard working solution concentration of each fat-soluble vitamin in table 3 is taken as an abscissa, the corresponding detected chromatographic peak area is taken as an ordinate, and the standard curve of each vitamin is prepared, and the linear range and the linear correlation coefficient r of each fat-soluble vitamin are shown in table 4.
The standard solution of the vitamin standard is diluted by using a blank matrix solution until the peak height of the compound is slightly more than 10 times of the signal to noise ratio as the quantitative limit of the method, and the quantitative limit of each fat-soluble vitamin is between 1 mug/100 g and 20 mug/100 g as shown in table 4.
TABLE 4 Linear Range, correlation coefficient and quantitative Limit Table
The results show that vitamin A, vitamin A palmitate, vitamin A acetate, vitamin E acetate and vitamin D 3 And vitamin K 1 Has good linear relation with the corresponding chromatographic peak area. Thus, according to the linear relation between the standard working solution concentration and the chromatographic peak area, the concentration of the milk powder sample to be measured can be calculated by measuring the chromatographic peak area of the sample to be measured.
2. Recovery rate and precision
And respectively carrying out a mark adding recovery experiment in a blank milk powder matrix. According to the content range of each fat-soluble vitamin in the formula milk powder sample, the adding level of each vitamin is set, wherein the low point of the standard adding concentration point is about 0.5 times of the average adding amount of the fat-soluble vitamin in the infant milk powder, the middle point is about 1.5 times of the average adding amount of the fat-soluble vitamin in the infant milk powder, each standard adding level is repeated for 6 times, the recovery rate and the precision test result of each fat-soluble vitamin in the milk powder matrix are shown in Table 5, the total recovery rate is between 81.7% and 99.8%, the relative standard deviation is between 1.13% and 6.33%, and the verification result shows that the detection method has better accuracy and precision.
TABLE 5 recovery and precision of fat-soluble vitamins in milk powder matrices
Example 6 measurement of actual infant milk powder sample
The fat-soluble vitamins of 5 infant formula milk powder seeds in different batches are detected by adopting the detection method, the content of each fat-soluble vitamin is calculated according to a standard curve, and the detection results are shown in table 6.
TABLE 6 vitamin content detection of actual samples
*：mg/100g
In practical tests, vitamin a is not detected in infant milk powder, and probably because vitamin a is poor in stability, vitamin a acetate or vitamin a palmitate is mainly added in the infant milk powder production.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and scope of the invention.
Claims (7)
1. The method for detecting the fat-soluble vitamins in the infant milk powder is characterized by simultaneously detecting the vitamin content in the infant milk powder by adopting liquid chromatography-mass spectrometry, and comprises the following steps of:
(1) Pre-treating a milk powder sample to be tested;
(2) Preparing standard working solution for establishing a standard curve;
(3) Detecting a milk powder sample to be detected by adopting a liquid chromatograph-tandem mass spectrometer;
wherein the fat-soluble vitamins include vitamin A and vitamin D 3 Vitamin E and vitamin K 1 The method comprises the steps of carrying out a first treatment on the surface of the The vitamin A also comprises the existing forms of vitamin A palmitate and vitamin A acetate, and the vitamin E also comprises the existing forms of vitamin E acetate;
conditions of the liquid chromatography: adopting a gradient elution mode, and a mobile phase A: 0.1.+ -. 0.05% formic acid solution, mobile phase B: 1+/-0.1% methylene dichloride methanol solution; the gradient elution mode specifically comprises the following steps: 0 to 0.5 minutes, 20 percent of A is kept unchanged; 0.5-4 minutes, 20% A is linearly changed to 0% A; 4-8.5 minutes, 0% A remains unchanged; 8.51 min change to 20% A, hold for 2min.
2. The method of claim 1, wherein the mass spectrometry conditions are: an atmospheric pressure chemical ionization ion source (APCI), positive ionization mode, ion pairs and collision energy parameters of the mass spectrum are specifically shown in the following table;
3. the method according to claim 1, characterized in that the milk powder to be tested is subjected to a pretreatment step comprising: accurately weighing a milk powder sample to be measured, adding a proper amount of antioxidant, dissolving with water, adding methanol to precipitate protein, and extracting fat-soluble vitamins from the milk powder sample by using an organic extraction solvent; centrifuging, taking upper layer solution, blowing nitrogen to dry, performing solvent conversion by using a double-dissolving solvent, and filtering to obtain the liquid to be detected.
4. A process according to claim 3, wherein the extraction solvent is isooctane.
5. The method of claim 4, wherein the redissolving solvent is acetone.
6. A method according to claim 3, characterized in that the conversion with the redissolved solvent is followed by filtration with an organic filter membrane having a thickness of 0.22 μm.
7. The method according to any one of claims 1-6, wherein the standard curve is established by an external standard method, in particular: preparing vitamin A, vitamin A palmitate, vitamin A acetate and vitamin D 3 Vitamin E, vitamin E acetate and vitamin K 1 The standard working solution of (2) is detected by a liquid chromatograph-tandem mass spectrometer, the chromatographic peak area of each fat-soluble vitamin is taken as the ordinate, the concentration is taken as the abscissa, and the standard curve of each vitamin is drawn.
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